Adhesive and method of making the same



Patented June 29, 1943 2,322,886

UNITED STATES PATENT 'OFFI CE ADHESIVEANDBIZZIZQFZJOFWG THE Seymour G. Saunders, Bloomfield Hills, and Harry Morrison, Detroit, Mich" asalgnors to r Chrysler Corporation, Highland Park, Micln, a

corporation of Delaware No Drawings Application February 14, 1940, SerlalNo. 3181.84;

11 Claims. (Cl. 260-) This invention relates to an improved adhesive ingredients are preferablypresent inthe followand method of making the same. ing proportions by weight: asphalt 33.5 pounds, More particularly, the invention pertains to an rosin (colophony) 7.1 pounds, ester gum 7.1 improved adhesive which is adapted for use in pounds and Petropol 23.&pounds. This heating connecting together parts of aniassembly includ- 5 operation may be conducted in any suitable kettle ing rubber and rubber-like substances or numerin which the materials are thoroughly fused toous other materials such as wood,-. fiber, fabric, gether while substantially 28.5 pounds of rubber metal and the like. scrap, such as tire scrap or mechanical rubber One of the main objects of the invention is the scrap, are added in relatively small increments inclusion in an adhesive of this kind of a resinous over a period of twenty minutes. During this constituent adapted to set by polymerization and twenty minute period, the temperature of the which is thus not susceptible to softening under batch is raised from the above mentioned tem heatas are thermoplastic resins. perature to substantially 480 F. at the end of the; I

Another object of the invention is to provide addition of the scrap. The batch is vigorously in an adhesive of this character a hydrocarbon stirred throughout this portion of the process resinous constituent which imparts increased adand the heating and stirring is continued while hesive strength and increased wetting properties th batch is held at substantially 480 F. for that enable the use of the adhesive on materials thirty minutes after completion of the addition which have heretofore resisted wetting by nuof rubber scrap. At this stage inthe process, merous adhesives. I the material of the batch is fairly homogeneous A furtheri object of the invention is to provide and thin, an p d p ast ser n an adhes of his The fused mass is then allowed to cool to subkind which imparts Plastiity h to n its Set stantially 230 F. and to it is added a mixture of s ate Wh l making a marked increase in the fillers and accelerators such as iron oxide. sultackiness of the adhesive in its unset state. phur hydrated i nd zinc oxide. It has been An additional object of the invention is the found t t following proportions of fillers provision of a plasticising tackifier in a rubber and accelerators by weight may be added, t 1. cement type of adhesive which reduces the rubvantage, to one hundred pounds of t base fused ber content requirement of a composition of this material; iron 33 pounds, Sulphur 33 kind and which accommodates the use of larger hydrated mm 2.9 pounds and zinc oxlde 3 percentages of asphalt, thereby reducing the final pwnda The resulting batch is tin ously 90st 9 the materialstirred thereafter while heated from 320 F. to We have found'tha't the foreg-omg obJects 325 F. for substantially thirty minutes. After be accomplished and other advantages obtained this treatment, theresulting material has a heavy in the manufacture of adhesives by the 111001" 35 body pomtion therein of msin'nke material The thus reacted batch which constitutes the mercmny known as Pen-0pm", Petropolis any base of the adhesive, is then rapidly cooled by drocarbon polymer resulting from the polymerization of the di-olefine constituent of a hydrocarg z g g gj' fg f z f f g ig 5 bon distillate in the presence of a suitable poly- 4.0 coo ng m a b] merizing agent such as fullers earth or sulphuric solvent to a s ed consislteacy. ofA gilioiiil 0 1e 2%; acid. The resulting polymerization product is Vent may compnse a so u on ta 1 n 57 reduced under steam and vacuum distillation to naphthaethyl gi i gi subsl t a heavier consistency of from 60% to solids. by Weight of the nap h er 3 u r h This product has a high iodine value of or 45 hides such as aviation ga'so me an s m a y The above which denotes a hi h de ree of unsaturadmcarbons may be'used for this purpose tion. These products are obtaified by high temammmt of solvent added is optional and depends upon the desired viscosity. When naphtha and gggaliure cracking of hydrocarbons at 1000 F. or alcohol aria employs? t3 thengmtetlgal iderivefd Petro 1 me. be used to advantage in nuso after the st men one coo s s p 8 P merous ibber cements of diverse compositions. e stant a y 80% 0f the total One adhesive composition embodying the invenquantity of naphtha to be used and thereafter tion may be compounded by heating together alcohol n an amount eq to tant y asphalt, rosin, ester gum and Petropol to a temof the total quantity of naphtha is thoroughly perature of from 450 F. to 460 F. The foregoing as mixed with the naphtha cut product, the remaining 20% or the naphtha being added and thoroughly mixed thereafter.

In place of dissolving the above mentioned base material in a solvent, it may be dispersed in water for many types of applications. This may be accomplished by milling together suitable quantities of the base and reclaim rubber with subsequent addition of rosin and stearic acid. The milling operation is preferably continued until all lumps of rosin and stearic acid have disappeared. Rosin oil is then added to the milled mass and the latter is further milled for approximately ten minutes. Then a suitable quantity of trisodium phosphate is dispersed -throughout the resulting mass by further mixing. During the foregoing mixing operation, the mass is heated sumciently to facilitate intimate oommingling of the constituents thereof and at the end of the mixing operation following addition of trisodium phosphate, the temperature should be from substantially 150 F. to 160 'F.

'I'he proportions of the above mentioned constituents'may be varied. A suitable composition may, forexample, comprise the following pro- When using the above composition, substantially 295 parts by weight of water are added in increments of five parts each until about three quarters of the total quantity of water have been introduced. The temperature of the mill is preferably so controlled during the addition of water as to b substantially at room temperature when the last of the above increments of 'water is added. The mass become "puffed up in appearance at this stage of the process and operation of the mill is continued for about fifteen minutes. Then the remaining water is added in increments of five parts of the total. 'During addition of the first or second increments of water of the last quarter added, a phase shift occurs. Until this stage is reached, the water is dispersed in the base material, and after this stage the base material becomes dispersed in the water.

After the phase shift, the mill may be cooled more rapidly to from 50 F. to 60 F. at the time of addition to the last increment.

The foregoing dispersion is stable and can be thinned to any desired consistency.

The resulting cement may appear to have a.

relatively low viscosity immediately after the cutting operation but on standing for from tion. The reclaim serves to increase the viscosity of the cement and add body thereto while at the same time materially increasing its adresult in prolonging, the setting time requirements.

During setting of the above described cement, the Petropol polymerizes to a set condition and thus when set is not susceptible to softening by heat as are compounds that are of thermoplastic nature. By employing this form of resinous mathe cement without destroying the adhesive strength properties thereof, for the preserice of Petropol enables the use of much higher percentages of asphalt, thus permitting a reduction in the rubber content of the composition. Petropol also so modifies the rosin and the reslnates which result from the reactions between the rosin and the active agents of the accelerating and filling constituents as to prevent the resulting reaction product from brittle when the cement is int. set state.

Although specific proportions of the ingredients have been set forth in order to disclose a representative embodiment of the invention, it is obvious that various changes in the quantities of materials employed in the manufacture of the improved adhesive may be made.

Although but several specific embodiments of the invention have been herein described, it will be understood that various changes in the sequence of operations, steps and materials employed may be made without departing from the spirit of the invention.

We claim:

1. An adhesive comprising in its unset state a liquid vehicle and a solids content incorporated therein comprising a fused together mass of asphalt, resinous materialhaving a main portion comprising hydrocarbon polymers resulting from polymerization of the di-oleflne constituents of a hydrocarbon distillate and rubber.

2. An adhesive having a solids content comprising the reaction product of a mixture including iron oxide, sulphur, lime and zinc oxide with a fused together mass of asphalt, resinous material having a main portion comprising hydrocarbon polymers of a hydrocarbon distillate and rubber.

3. An adhesive having a solids content comprising the reaction product of a mixture including iron oxide, sulphur, lime and zinc oxide with a fused together mass of asphalt, resinous material having a main portion comprising-ester gum and hydrocarbon polymers resulting from polymerization of the di-olefine constituents of a hydrocarbon distillate and rubber.

4. An adhesive having a solids content comprising the reaction product of a fused mass of asphalt, rosin, ester gum, rubber scrap and hydrocarbon polymers resulting from polymerization of the di-olefine constituentsof a hydrocarbon distillate, with a combined filler and acceleheslve strength. The tackiness of the cement may be further increased by the addition ofcumar gum in an amount equal to substantially 10% of the weight of the batch immediately prior to the cutting operation. This addition may rator content.

5. A cement comprising the reaction product formed while in intimate mixture with iron and zinc oxides of a fused mass of asphalt, rubber and resinous material including a major portion of hydrocarbon polymers resulting from polymerization of the di-olefine constituents of a hydrocarbon distillate with sulphur and lime.

6. A cement comprising the reaction product of a fused fuming mass of asphalt, rubber and resinous material including a major portion ofhydrocarbon polymers resulting from polymerization of the di-olefine constituents of a hydrocarbon distillate with sulphur and lime, and a volatile vehicle.

7. A cement comprising the reaction product of a fused fuming mass of asphalt, rubber in the form of the scrap, and resinous material including a major portion of hydrocarbon polymers resulting from polymerization of the dl-olefine constituents of a hydrocarbon distillate with Sulphur and lime, said reaction product being formed while a metallic oxide accelerating agent is intimately mixed therewith.

8. A cement comprising the reaction product of a fused fuming mass of asphalt, rubber in the form of tire scrap, and resinous material including a major portion of hydrocarbon polymers resulting from polymerization of the di-oleflne constituents of a hydrocarbon distillate with sulphur and lime, said reaction product being formed while a metallic oxide accelerating agent is intimately mixed therewith and a plasticising constituent comprising cumar gum and reclaim rubber.

9. The method of making an adhesive composition which comprises the steps of fusing together asphalt, rosin, ester gum, rubber and a hydrocarbon polymer resulting from polymerization of di-olefine constituents of a hydrocarbon distillate, reacting the resulting product while in a fused state with iron oxide, sulphur, hydrated lime and zinc oxide, and diluting the final product with a volatile solvent.

10. The method of making an adhesive composition which comprises the steps of fusing together at from 450 F. to 460 F. asphalt, rosin, ester gum and hydrocarbon polymers resulting from polymerization of the di-olefine constitucuts of a hydrocarbon distillate, adding rubber scrap in comparatively small increments over a period of substantially twenty minutes during in- CROSS REFERENCE creasing of the temperature of the batch from said above mentioned value to substantially 480 F. at the end of said twenty minute period, continuing heating of said batch at said last mentioned temperature for substantially thirty minutes, cooling said batch thereafter to from 320 F. to 325 F., introducing a mixture of iron oxide, sulphur, hydrated lime and zinc oxide into said batch and maintaining the temperature of the combined batch at 320 F. to 325 F. for substantially thirty minutes, rapidly cooling the resulting product thereafter, and cutting said product in a volatile vehicle.

11. The method of making an adhesive composition which comprises the steps of fusing together at from 450 F. to 460 F. asphalt 33.5 parts by weight, rosin 7.1 part by weight, ester gum 7.1 parts by weight and hydrocarbon polymers resulting from polymerization of the di-olefine constituents of a hydrocarbon distillate 23.5 parts by weight; adding 28.5 parts by weight of rubber scrap in small increments over a period of substantially thirty minutes during increasing of the temperature of th resulting batch to substantially 480 F. at the end of said twenty minute period; continuing heating of said batch at said last mentioned temperature for substantially thirty minutes; cooling said batch thereafter to substantially 320 F.; introducing into each lbs. of said batch a mixture comprising 3.8 pounds of iron oxide, 3.3 pounds of sulphur, 2.9 pounds of hydrated lime and 2.9 pounds of zinc oxide and maintaining the temperature of said batch at 320 F. to 325 F. for substantially thirty minutes; cooling the resulting product thereafter to normal atmospheric temperature, and cutting said product in a volatile vehicle.

SEYMOUR G. SAUNDERS. HARRY MORRISON.

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